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Dicyclohexylcarbodiimide → HCID 178444060、化合物

HRID 2226077
ノート
印刷プレビュー

反応式

HRID 2226077 の反応式
[F:1][C:2]1[C:10]([F:11])=[C:9]([O:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[CH2:20]([C@H:25]1[CH2:30][CH2:29][C@H:28]([CH2:31][CH2:32][CH2:33][CH2:34][C:35]2[CH:40]=[CH:39][C:38](O)=[CH:37][CH:36]=2)[CH2:27][CH2:26]1)[CH2:21][CH2:22][CH2:23][CH3:24].C1(N=C=NC2CCCCC2)CCCCC1>CN(C)C1C=CN=CC=1.ClCCl>[CH2:20]([C@H:25]1[CH2:30][CH2:29][C@H:28]([CH2:31][CH2:32][CH2:33][CH2:34][C:35]2[CH:36]=[CH:37][C:38]([O:5][C:4](=[O:6])[C:3]3[CH:7]=[CH:8][C:9]([O:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19])=[C:10]([F:11])[C:2]=3[F:1])=[CH:39][CH:40]=2)[CH2:27][CH2:26]1)[CH2:21][CH2:22][CH2:23][CH3:24]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 10868DicyclohexylcarbodiimideHCID 189659312,3-Difluoro-4-heptyloxybenzoic acidHCID 178444450HCID 178444450、化合物

生成物 1

HCID 178444060HCID 178444060、化合物収率 54.3%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒
HCID 6344
Dichloromethane
溶媒

実験手順

1.9 g of 2,3-difluoro-4-heptyloxybenzoic acid, 2 g of 4-[4-(trans-4-pentylcyclohexyl)-1-butyl]phenol and 0.1 g of 4-(dimethylamino)pyridine were dissolved in 250 ml of dichloromethane and the solution was treated portionwise within 10 minutes while stirring with 1.6 g of N,N'-dicyclohexylcarbodiimide. The mixture was stirred at room temperature overnight and then filtered. The filtrate was diluted with dichloromethane, washed twice with 50 ml of saturated sodium carbonate solution each time and then with water, dried over magnesium sulfate, filtered and then concentrated. Chromatography of the residue on silica gel with toluene/ethyl acetate (vol. 4:1) and recrystallization from ethanol gave 2 g of 2,3-difluoro-4-heptyloxybenzoic acid 4-[4-(trans-4-pentylcyclohexyl)-1-butyl]phenyl ester with m.p. (C-SC) 67° C., SC -N 70° C. and cl.p. (N-I) 128° C.

後処理

  1. additionthe solution was treated portionwise within 10 minutes
  2. filtrationfiltered
  3. additionThe filtrate was diluted with dichloromethane
  4. washwashed twice with 50 ml of saturated sodium carbonate solution each time
  5. dry with materialwith water, dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customChromatography of the residue on silica gel with toluene/ethyl acetate (vol. 4:1) and recrystallization from ethanol

出典と根拠

ORDレコード
ord-848f5003d9e94bc7a660667df16d53ed
出典データセット
uspto-grants-1994_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05346647

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート